HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 67922668, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 4-Chlorobutyryl chloride | HCID 78370 | — |
| Reactant | HCID 67922774 | HCID 67922774 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67922668 | HCID 67922668 | 100% |
Reaction Steps
To a stirred and cooled (ice/bath) mixture of 7.9 parts of cis-3-methoxy-N,N-dimethyl-4-piperidinamine, 7 parts of N,N-diethylethanamine, 195 parts of dichloromethane were added dropwise 6.16 parts of 4-chlorobutanoyl chloride (temperature <5° C.). Upon completion, stirring was continued for 30 minutes. The organic layer was washed twice with a saturated sodium chloride solution, dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (90:10 by volume) as eluent. The pure fractions were collected and the eluent was evaporated, yielding 13.7 parts (100%) of cis-1-(4-chloro-1-oxobutyl)-3-methoxy-N,N-dimethyl-4-piperidinamine (int. 29).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05041454 |
| Source dataset | uspto-grants-1991_08 |
| ORD ID | ord-3c6fc9dd2b4840a5b0fc0086c2a44e2c |
| Source note | uspto-grants-1991_08 |